CN103803985A - Preparation method of cubic boron nitride and diamond polycrystal with nanometer structure - Google Patents
Preparation method of cubic boron nitride and diamond polycrystal with nanometer structure Download PDFInfo
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 61
- 239000010432 diamond Substances 0.000 title claims abstract description 60
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 54
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052796 boron Inorganic materials 0.000 claims abstract description 31
- 239000011812 mixed powder Substances 0.000 claims abstract description 21
- 239000002086 nanomaterial Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000013590 bulk material Substances 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 239000011230 binding agent Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 239000002113 nanodiamond Substances 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 26
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 16
- 239000003595 mist Substances 0.000 description 12
- 239000007858 starting material Substances 0.000 description 9
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- 238000004062 sedimentation Methods 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 229910052715 tantalum Inorganic materials 0.000 description 5
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 5
- 229910001868 water Inorganic materials 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 3
- 229910001573 adamantine Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
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- 229910017604 nitric acid Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种新型纳米结构立方氮化硼—金刚石聚晶的制备技术。采用六方氮化硼与金刚石混合粉末或立方氮化硼与金刚石混合粉末为原材料，原材料中金刚石所占质量分数为10%—90%。经净化除杂后，不添加任何粘结剂，装配烧结单元，直接经高温超高压烧结制备纳米结构立方氮化硼—金刚石聚晶。这种纳米结构立方氮化硼—金刚石聚晶，物相分布均匀，立方氮化硼晶粒为纳米尺寸，金刚石晶粒均匀分布在纳米立方氮化硼晶粒中，大面积形成结合紧密、高强度的纳米立方氮化硼—金刚石界面。这使得本发明的高性能纳米结构立方氮化硼—金刚石聚晶的硬度与金刚石单晶硬度相当，热稳定性，硬度，及耐磨性也明显优于含金属粘结剂的金刚石聚晶。
The invention relates to a novel nanostructure cubic boron nitride-diamond polycrystal preparation technology. The mixed powder of hexagonal boron nitride and diamond or the mixed powder of cubic boron nitride and diamond is used as the raw material, and the mass fraction of diamond in the raw material is 10%-90%. After purification and removal of impurities, no binder is added, the sintering unit is assembled, and the nanostructured cubic boron nitride-diamond polycrystal is directly sintered at high temperature and ultra-high pressure. This nano-structured cubic boron nitride-diamond polycrystal has uniform phase distribution, cubic boron nitride grains are nano-sized, and diamond grains are evenly distributed in nano-cubic boron nitride grains. Strength of nanocubic boron nitride-diamond interface. This makes the hardness of the high-performance nanostructured cubic boron nitride-diamond polycrystal of the present invention comparable to that of diamond single crystal, and its thermal stability, hardness, and wear resistance are also significantly better than those of diamond polycrystal containing metal binders.
Description
The present invention relates to a kind of take hexagonal boron nitride and diamond mixed powder or cubic boron nitride and diamond mixed powder as starting material, pass through purifying treatment, the method of preparing high performance and nano structure cubic boron nitride-dimond synneusis superhard material under superhigh-pressure high-temp condition, belongs to field of inorganic nonmetallic material.
Technical background
Diamond and cubic boron nitride are most widely used two kinds of superhard materials in current industry.Diamond is occurring in nature the hardest known material, there is high wear resistance, ultimate compression strength, rate of heat release, diamond single crystal is expensive and have the face of dissociating, and in industry, a lot of fields replace diamond single crystal with the higher polycrystalline diamond material of cost performance.Polycrystalline diamond is widely used in non-ferrous metal and the machining of iron containing alloy not, and oil and gas and mining industry are surveyed and adopted, wood floors processing and other fields.The hardness of cubic boron nitride is about adamantine half, to be only second to adamantine the second hard material, but cubic boron nitride has the thermostability higher than diamond and is difficult for and ferro element generation chemical reaction, thereby can be used for processing ferrous metal or iron containing alloy, cubic boron nitride monocrystal is expensive and have the face of dissociating, and in industry, a lot of fields replace cubic boron nitride monocrystal by the higher Polycrystalline Cubic Boron Nitride of cost performance.Polycrystalline cubic boron nitride is owing to having higher red hardness, compared with high wear resistance and high thermostability and be widely used in the machining of ferrous metal and iron containing alloy.
Cubic boron nitride-dimond synneusis material has been taken into account the advantage of polycrystalline diamond and polycrystalline cubic boron nitride, cubic boron nitride-dimond synneusis sintered compact that system passes is after adding the metal-powders such as (or not adding direct sintering) Co, Ni, TiC, TiN evenly to mix in artificial cubic boron nitride and diadust, a kind of super-hard compound material that sintering forms under high pressure-temperature, it shows isotropy and higher hardness and toughness in macroscopic view, and application performance is in some aspects better than polycrystalline diamond and polycrystalline cubic boron nitride.But traditional artificial cubic boron nitride-dimond synneusis material, because granularity is larger, is difficult to reach planeness and the sharpness for hyperfine cutting tool cutting edge.In addition, traditional artificial cubic boron nitride-dimond synneusis material contains binding agent mostly, as Co, Ni etc., has a strong impact on hardness, wear resistance, the thermostability of cubic boron nitride-dimond synneusis material.
Utilizing hexagonal boron nitride and diamond mixed powder or cubic boron nitride and diamond mixed powder is starting material, prepares reporting for work of high performance and nano structure cubic boron nitride-dimond synneusis and also do not occur under superhigh-pressure high-temp.
Summary of the invention
The object of the invention is in order to overcome the deficiency in above-mentioned traditional man-made polycrystalline diamond, polycrystalline cubic boron nitride, cubic boron nitride-dimond synneusis material preparation technology, disclose a kind ofly take hexagonal boron nitride and diamond mixed powder or cubic boron nitride and diamond mixed powder as starting material, in starting material, the shared massfraction of diamond is 10%-90%.By to starting material purifying treatment, under superhigh-pressure high-temp, prepare the method for high performance and nano structure cubic boron nitride-dimond synneusis material.
The method of nanostructure cubic boron nitride-dimond synneusis material of preparation of the present invention is carried out in accordance with the following steps:
One, removal of impurities, obtains high purity hexagonal boron nitride and diamond mixed powder or cubic boron nitride and diamond mixed powder original material.If raw material itself is very pure, can no longer carry out this step.The technical process of removal of impurities is: acid-soluble, powder liquid separating, washing, heating, drying three process continuously.The wherein kind of acid, concentration and can suitably changing as the case may be with the ratio of raw material.
A. acid-soluble continuously: raw material is placed in polytetrafluoroethylcontainer container by (1), adding concentration is the hydrofluoric acid of 20%-40%, the add-on ratio of hydrofluoric acid and raw material micro mist is 1-2 ml/g and draws (ml/ct), suitable heating in water bath (20-100 ℃) to use whipping appts continuously stirring, treatment time be 72 hours when acid-soluble.After being disposed, treat that micro mist sedimentation is complete, remove liquid, and repeat to be diluted to approaching neutral with deionized water.(2) the raw material micro mist after hydrofluoric acid treatment is placed in to glass beaker, adding concentration is the hydrochloric acid of 20%-38%, or to add concentration be the nitric acid of 30%-50%, acid is 1-2 ml/g with the add-on ratio of raw material micro mist and draws (ml/ct), suitable heating in water bath (20-100 ℃) to use whipping appts continuously stirring, treatment time be 72 hours when acid-soluble.After being disposed, treat that micro mist sedimentation is complete, remove liquid, and repeat to be diluted to approaching neutral with deionized water.
B. powder liquid separating, washing: continuous acid-soluble removal of impurities and be diluted to neutrality after, in beaker, sedimentation raw material micro mist, removes liquid after sedimentation, leaves raw material micro mist.
C. heating, drying: the raw material micro mist staying in beaker is put into process furnace and carry out drying and processing, treatment temp is 70 ℃, until dry.
Two, vacuum high-temperature processing: the raw material micro mist after acid-soluble removal of impurities is displayed with corundum crucible, and by cap covers, put into vacuum oven treating chamber.When processing, guarantee that vacuum tightness is better than 4x10
-3pa, temperature is 500-1000 ℃, the treatment time is 1-3 hour.
Three, assembling sintering unit: grinding and buffing lapping tantalum paper tinsel surface, deoil, ultrasonic cleaning, infrared drying.Raw material micro mist after treatment and purification is put into parcel, after pre-molding, put into the sample cavity of high-pressure synthesizer.
Four, High Temperature High Pressure sintering: sintering pressure is 8-20GPa, heats when pressurize, and sintering temperature is 1000-2700 ℃, insulation 10-30 minute.After insulation, slow cooling, to 300-500 ℃, starts step-down.In step-down process, keeping temperature is 300-500 ℃.
Five, following process: sample is put into 30% hydrofluoric acid 20ml and 40% nitric acid 20ml mixing acid is removed lapping tantalum, adopt diamond disk polishing sample to light.
The invention has the advantages that:
Nanostructure cubic boron nitride-dimond synneusis material of the present invention, adopting hexagonal boron nitride and diamond mixed powder or cubic boron nitride and diamond mixed powder is raw material, utilize superhigh-pressure high-temp condition, the cubic boron nitride that hexagonal boron nitride in starting material is become in cubic boron nitride or the starting material of nanostructure is mutually broken for nanocrystal through high pressure, massfraction is that 10%-90% diamond crystals is evenly distributed in nano cubic boron nitride crystal grain as hardness wild phase, big area forms in conjunction with tight, high-intensity nano cubic boron nitride-diamond interface, finally sinter nanostructure cubic boron nitride-dimond synneusis into.This high-performance polycrystalline diamond material does not add metal adhesive, but utilize superhigh-pressure high-temp condition, make material thing mutually only containing diamond and cubic boron nitride, and by the control of pressure and temperature, make hexagonal boron nitride in starting material become mutually the cubic boron nitride of nanostructure or nanocrystal that cubic boron nitride is broken into through high pressure is no longer grown up.
The hardness of high performance and nano structure cubic boron nitride-dimond synneusis of the present invention and natural diamond single crystal hardness are suitable, and thermostability and cutting ability are also obviously better than the traditional man-made diamond glomerocryst containing binding agent.This material not only can be used as ordinary cutting tool material, also can be used as superhigh precision cutter material.
The present invention is high performance and nano structure cubic boron nitride-dimond synneusis of preparing under the superhigh-pressure high-temp condition of utilizing domestic hinge type six-plane piercer to produce.Hinge type six-plane piercer is to produce at present diadust, the major equipment of sintering tradition man-made diamond glomerocryst.The present invention can be on the basis of existing installation, prepares on a large scale high performance and nano structure cubic boron nitride-dimond synneusis material.
Below by the drawings and specific embodiments, the present invention will be further described, but and do not mean that limiting the scope of the invention.
Accompanying drawing explanation
Accompanying drawing 1 process flow sheet of the present invention:
Accompanying drawing 2 sintering unit wiring layouts:
In accompanying drawing, the object of each label mark is:
1 agalmatolite, 2 rhombspars, 3 thermopairs, 4 graphite, 5 steel bowls, 6 titanium sheets, 7 samples, 8, vitrified pipe 9, tantalum cup
Embodiment
Below by embodiment, the present invention is specifically described; be necessary to be pointed out that at this present embodiment is only further described for the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1:
Selecting median size is that diamond and the mean particle size of 0-2 μ m is the hexagonal boron nitride mixed powder of 0-2 μ m, wherein adamantine massfraction is 85%, prepares high performance and nano structure cubic boron nitride-dimond synneusis material according to the process flow sheet shown in Fig. 1.It is that the hydrofluoric acid of 20%-40% is processed that diamond and hexagonal boron nitride mixed powder are first put into concentration.The add-on ratio of hydrofluoric acid and admixed finepowder is 2 mls/g and draws (ml/ct), and 70 ℃ of heating in water bath, and continuously stirring are processed 72 hours.After being disposed, treat that micro mist sedimentation is complete, remove liquid, and repeat to be diluted to approaching neutral with deionized water.Admixed finepowder after hydrofluoric acid treatment is placed in to the hydrochloric acid that concentration is 20%-38%, and acid is 2 mls/g with the add-on ratio of admixed finepowder and draws (ml/ct), 70 ℃ of heating in water bath continuously stirring, and the treatment time is 72 hours.After being disposed, treat that micro mist sedimentation is complete, remove liquid, and repeat to be diluted to approaching neutral with deionized water.Acid-soluble removal of impurities process is carried out after 3-5 time repeatedly above, and sedimentation admixed finepowder in beaker, removes liquid after sedimentation, leave admixed finepowder.The admixed finepowder staying is put into process furnace and carry out drying and processing, treatment temp is 70 ℃, until dry.Carry out again vacuum high-temperature processing, the admixed finepowder after removal of impurities is displayed with corundum crucible, and by cap covers, put into vacuum oven treating chamber.Processing vacuum tightness is 4x10
-3pa, temperature is 800 ℃, processes 1 hour, removes the impurity such as oxygen, nitrogen, water vapour of diamond surface absorption.
According to sintering unit wiring layout assembling sintering unit, as shown in Figure 2.First grinding and buffing lapping (9) tantalum paper tinsel surface, deoils, ultrasonic cleaning, infrared drying processing.Diamond after purifying treatment and hexagonal boron nitride admixed finepowder are put into parcel, pre-molding, and according to wiring layout assembling sintering unit group.When High Temperature High Pressure sintering, sintering pressure is 1GPa, and sintering temperature is 1800 ℃, and sintering time is 10 minutes.After decrease temperature and pressure, sample is put into 30% hydrofluoric acid 20ml and 40% nitric acid 20ml mixing acid is removed lapping tantalum, adopt diamond disk polishing sample to light.
Adopt high performance and nano structure cubic boron nitride-dimond synneusis material thing prepared by this technique only to contain mutually diamond and cubic boron nitride, and by the control of pressure and temperature, make hexagonal boron nitride in starting material become mutually the cubic boron nitride of nanostructure or nanocrystal that cubic boron nitride is broken into through high pressure is no longer grown up, this material has high rigidity and density, high thermostability, wear resistance and toughness are the novel superhard materials that a kind of performance is very superior.
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| CN104440605A (en) * | 2014-11-11 | 2015-03-25 | 河南富耐克超硬材料股份有限公司 | Polygonal superhard abrasive compound and method for manufacturing abrasive tool with same |
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